EP1746186A1 - Procede de fabrication d'un monocristal de silicium et monocristal de silicium - Google Patents

Procede de fabrication d'un monocristal de silicium et monocristal de silicium Download PDF

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Publication number
EP1746186A1
EP1746186A1 EP05727712A EP05727712A EP1746186A1 EP 1746186 A1 EP1746186 A1 EP 1746186A1 EP 05727712 A EP05727712 A EP 05727712A EP 05727712 A EP05727712 A EP 05727712A EP 1746186 A1 EP1746186 A1 EP 1746186A1
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EP
European Patent Office
Prior art keywords
carbon
organic compound
single crystal
silicon
silicon single
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EP05727712A
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German (de)
English (en)
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EP1746186A4 (fr
EP1746186B1 (fr
Inventor
R. c/o Shirakawa R & D Center HOSHI
Naoki; c/o Shirakawa R & D Center NAGAI
Izumi; c/o Shirakawa R & D Center FUSEGAWA
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Shin Etsu Handotai Co Ltd
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Shin Etsu Handotai Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon

Definitions

  • the present invention relates to a method for producing a silicon single crystal from which a silicon wafer, used as a substrate of a semiconductor device such as memory or CPU, is sliced and, more particularly, to a method for producing a silicon single crystal and a silicon single crystal used in front-end technology in which crystal defects and density of BMD for gettering impurities are controlled by carbon-doping.
  • a silicon single crystal is produced mainly by the Czochralski method (Hereinafter, the Czochralski method is abbreviated to the CZ method).
  • a silicon wafer is sliced from the silicon single crystal, and is used as a substrate of a semiconductor device such as memory or CPU.
  • a silicon single crystal produced by the CZ method contains oxygen atoms.
  • a silicon atom and oxygen atoms are bonded together to form oxide precipitates (Bulk Micro Defect; Hereinafter, it is abbreviated to BMD).
  • BMD has the IG (Intrinsic Gettering) capability to catch contamination atoms such as heavy metal in a wafer and to improve device characteristics. Higher concentration of BMD in the bulk of a wafer provides a higher performance device.
  • gas doping See Japanese Unexamined Patent Application Publication No. H11-302099
  • use of high purity carbon powder See Japanese Unexamined Patent Application Publication No. 2002-293691
  • use of carbon blocks See Japanese Unexamined Patent Application Publication No. 2003-146796
  • the above methods have problems, respectively.
  • the gas doping remelting a crystal is impossible when the crystal is dislocated.
  • high purity carbon powder introduced gas scatters the high purity carbon powder at the time of melting material.
  • carbon blocks carbon is hard to melt and a crystal being grown is dislocated.
  • Japanese Unexamined Patent Application Publication No. H11-312683 suggests a method to dope a silicon single crystal with carbon by putting a polycrystalline silicon container containing carbon powder, a silicon wafer on which a carbon film is vapor-deposited, a silicon wafer on which an organic solvent containing carbon particles is applied and baked, or polycrystalline silicon with a certain content of carbon in a crucible.
  • Use of these methods overcomes the problems.
  • every method requires a process of polycrystalline silicon, a heat treatment of a wafer, and so on. Consequently, it is not easy to prepare a carbon dopant.
  • the process or the heat treatment of a wafer for preparing the carbon dopant can cause contamination by impurities.
  • Japanese Unexamined Patent Application Publication No.2001-199794 and International Publication No.01/79593 disclose a method for obtaining a silicon single crystal with few grown-in defects and with high IG capability by doping the crystal with carbon and nitrogen together. Doping a silicon single crystal with nitrogen is conducted commonly by mixing a wafer on the surface of which a silicon nitride film is formed into a polycrystalline material (see Japanese Unexamined Patent Application Publication No.H05-294780 ). However, such methods cannot overcome the above problems in carbon-doping.
  • the present invention is accomplished in view of the aforementioned problems, and its object is to provide a method for producing a silicon single crystal with carbon-doping in which the crystal can be doped with carbon easily at low cost, and carbon concentration in the crystal can be controlled precisely.
  • a method for producing a silicon single crystal by the Czochralski method with carbon-doping comprising: charging a polycrystalline silicon material and any one of a carbon dopant selected from the group consisting of an organic compound, an organic compound and a silicon wafer, carbon powder and a silicon wafer, an organic compound and carbon powder, and an organic compound and carbon powder and a silicon wafer into a crucible and melting the polycrystalline silicon material and the carbon dopant; and then growing a silicon single crystal from the melt of the polycrystalline silicon material and the carbon dopant.
  • a polycrystalline silicon material and any one of a carbon dopant selected from the group consisting of an organic compound, an organic compound and a silicon wafer, carbon powder and a silicon wafer, an organic compound and carbon powder, and an organic compound and (carbon powder and a silicon wafer are charged into a crucible. And the polycrystalline silicon material and the carbon dopant are melted. After that, a silicon single crystal is grown from the melt of the polycrystalline silicon material and the carbon dopant. As a result, a silicon single crystal can be doped with carbon easily and precisely.
  • the carbon dopant selected from the group consisting of the organic compound and the silicon wafer, the carbon powder and the silicon wafer, and the organic compound and the carbon powder and the silicon wafer is charged into the crucible with sandwiching the organic compound and/or the carbon powder between a plurality of the silicon wafers.
  • the carbon dopant selected from the group consisting of the organic compound and the silicon wafer, the carbon powder and the silicon wafer, and the organic compound and the carbon powder and the silicon wafer when the organic compound and/or the carbon powder is sandwiched between a plurality of the silicon wafers, the organic compound and the carbon powder are put between the silicon wafers. Furthermore, in the case of using the organic compound and the silicon wafer, the organic compound adheres to the silicon wafer at the time of melting material. Consequently, material melt is more certainly doped with elements of the organic compound. In addition, in the case of using the carbon powder, it can be prevented that an introduced inert gas such as argon gas scatters the carbon powder at the time of melting material. Therefore, it becomes possible to control carbon concentration in the material melt to be a desired concentration.
  • an introduced inert gas such as argon gas scatters the carbon powder at the time of melting material. Therefore, it becomes possible to control carbon concentration in the material melt to be a desired concentration.
  • the carbon dopant selected from the group consisting of the organic compound and the carbon powder, and the organic compound and the carbon powder and the silicon wafer is charged into the crucible with containing the carbon powder in a bag made of the organic compound.
  • main elements of the organic compound consist of carbon and hydrogen, or carbon and hydrogen and oxygen.
  • a silicon crystal can be doped with carbon by the use of the organic compound in which main elements consist of carbon and hydrogen, or carbon and hydrogen and oxygen. And, the elements except carbon have an advantage that such elements do not become impurities having harmful effects to silicon characteristics even when the elements are melted into a silicon single crystal.
  • the organic compound may include carbon and nitrogen as main elements.
  • a silicon single crystal can be doped with nitrogen in addition to carbon.
  • Any one or more of polyethylene, vinyl polymer and nylon can be used as the organic compound.
  • the present invention also provides a carbon-doped silicon single crystal produced by the method for producing a silicon single crystal according to the present invention.
  • the method for producing a silicon single crystal according to the present invention provides a carbon-doped silicon single crystal with a desired carbon concentration.
  • the present invention overcomes the problems that an inert gas scatters a carbon dopant at the time of melting material, and so on. Consequently, carbon concentration in a silicon single crystal can be controlled to be a target value precisely, and a carbon-doped silicon single crystal can be produced easily at low cost. Furthermore, the present invention enables doping of carbon and nitrogen together. Such a carbon- and nitrogen-doping provides excellent control of carbon- and nitrogen concentration, and can be carried out with extreme ease at low cost.
  • Fig.1 shows an example of an apparatus for pulling a single crystal used in carrying out a method for producing a carbon-doped silicon single crystal according to the present invention.
  • a quartz crucible 5 and a graphite crucible 6 are provided in a main chamber 1 of an apparatus 20 for pulling a single crystal.
  • the quartz crucible 5 contains a melted material melt 4.
  • the graphite crucible 6 supports the quartz crucible 5.
  • the graphite crucible 6 is surrounded by a heater 7. Further, insulating material 8 surrounds the outside of the heater 7. Further, over the material melt 4, a gas flow-guide cylinder 11 and a heat insulating component 12 are provided to surround a silicon single crystal 3.
  • polycrystalline silicon and a carbon dopant which are materials for a carbon-doped silicon single crystal according to the present invention, are charged. At this time, a dopant for controlling resistivity of a substrate such as phosphorus or boron is added.
  • the carbon dopant used in the present invention is any one selected from the group consisting of an organic compound; an organic compound and a silicon wafer; carbon powder and a silicon wafer; an organic compound and carbon powder; and an organic compound and carbon powder and a silicon wafer.
  • the organic compound a compound having main elements of carbon and hydrogen, or carbon and hydrogen and oxygen such as polyethylene or vinyl polymer is used. Use of such an organic compound has a great advantage of not causing problems in growing a single crystal.
  • the carbon powder is not particularly limited by purity or grain size.
  • carbon powder with high purity is preferably used because use of the powder reduces generation of defects such as OSF due to impurities contained in the carbon powder.
  • the carbon powder with high purity is, for example, carbon powder with purity of 99.99% or more and with ash content of 0.01% or less.
  • the carbon dopant is preferably charged together with polycrystalline silicon 15 into the quartz crucible 5 with sandwiching the organic compound 17 and/or the carbon powder 18 between a plurality of the silicon wafers 16.
  • Fig.2 shows an example of sandwiching with two silicon wafers. However, more wafers may be used in accordance with an amount of the organic compound 17 or the carbon powder 18.
  • an expensive wafer such as a polished wafer is not necessarily used.
  • a chemical etched wafer and so on satisfies the requirements.
  • surface conditions of a wafer a level similar to that of an as-sliced wafer satisfies the requirements as long as surface cleanliness has no problem. Such wafers are available at lower cost.
  • the materials are charged into the quartz crucible 5. Then, Ar gas is introduced from a gas inlet 10 set in a pulling chamber 2, while air is exhausted from a gas outlet 9 by running a vacuum pump (not shown). In this way, the internal atmosphere is replaced with Ar atmosphere.
  • the heater 7 surrounding the graphite crucible 6 heats and melts the materials to obtain the material melt 4.
  • an organic compound 17 adheres to the silicon wafers 16 at the time of being melted. Or, when the organic compound 17 evaporates, the compound 17 is certainly caught by the silicon wafers 16. Then, the silicon wafers 16 are melted, and elements of the organic compound 17 are also melted into the melt 4. Thus the melt 4 is doped with carbon.
  • sandwiching the powder 18 between the silicon wafers 16 prevents Ar gas from scattering the powder 18 during melting. And the powder 18 is melted into the material melt 4. In this manner, because carbon is kept from scattering at the time of melting, it becomes possible to control carbon concentration in the material melt 4 to be a desired concentration.
  • a seed crystal 13 is immersed into the material melt 4. Then the seed crystal 13 is pulled upwardly with being rotated to grow a rod-like silicon single crystal 3. Thus a carbon-doped silicon single crystal with a desired carbon concentration is produced.
  • an organic compound such as polyethylene or vinyl polymer is processed into a bag. Then carbon powder is contained in the bag to prepare a carbon dopant. Together with polycrystalline silicon and a dopant controlling resistivity, the carbon dopant is charged into a quartz crucible. Then the materials are melted and a crystal is grown as is the case with above. Thus a carbon-doped silicon single crystal with a desired carbon concentration is produced.
  • a bag made of an organic compound containing carbon powder may be charged into a quartz crucible also with sandwiching the bag between silicon wafers. Use of such a method prevents the carbon powder and so on from scattering more certainly.
  • the method for producing a silicon single crystal with carbon-doping by using an organic compound consisting of carbon and hydrogen, or carbon and hydrogen and oxygen such as polyethylene or vinyl polymer was explained above.
  • the present invention may use an organic compound including carbon and nitrogen as main elements such as nylon.
  • carbon and nitrogen as main elements such as nylon.
  • nitrogen is melted into a material melt at the time of melting material.
  • pulling a crystal from such a material melt provides a carbon- and also nitrogen-doped silicon single crystal. Consequently, use of such a method enables easy carbon- and nitrogen-doping, and a carbon- and nitrogen-doped silicon single crystal with high purity can be produced at low cost.
  • Example 1 Comparative Example Average Value of Carbon Concentration (x 10 16 atoms/cc New ASTM) 3.06 3.01 2.82 ⁇ 0.20 0.12 0.32 Average Value of Lifetime ( ⁇ sec) 582 580 560 ⁇ 38 45 44
  • P-type silicon single crystals were produced with the same conditions as Example 1, except charging high purity carbon powder sandwiched between two chemical etched silicon wafers as a carbon dopant into a quartz crucible.
  • high purity carbon powder carbon powder with purity of greater than 99.99%, with ash content of less than 0.01%, and with a particle diameter of 1 to 100 ⁇ m was used.
  • Wafer-shaped samples were sliced from the silicon single crystals at 100 cm from the top of the straight body, respectively. Carbon concentration and lifetime of the samples were measured.
  • Example 1 Five P-type silicon single crystals were produced with the same conditions as Example 1 and Example 2, except charging the same high purity carbon powder as Example 2 directly without being sandwiched between wafers, together with a polycrystalline silicon material, into a quartz crucible. Wafer-shaped samples were sliced from the silicon single crystals at 100 cm from the top of the straight body, respectively. Carbon concentration and lifetime of the samples were measured.
  • Example 1 and 2 achieved the carbon concentrations almost the same as the target value. Moreover, deviations of carbon concentrations among five samples were small. On the other hand, in Comparative Example 1, the average value of carbon concentrations of five samples was less than those of Example, and the deviation was larger than those of Examples. In addition, in Comparative Example, there were many dislocations of the crystals, and it took more time to produce a silicon single crystal by about 30% on average than Examples.
  • the production method according to the present invention provides a silicon single crystal with a desired carbon concentration and with stability.
  • a P-type silicon single crystal with a diameter of 300 mm and with a straight body length of 140 cm was grown with applying horizontal magnetic field at a central magnetic field intensity of 3000 G by the MCZ (Magnetic field applied czochralski) method. After that, a wafer-shaped sample was sliced from the crystal at 140 cm from the top of the straight body. Carbon concentration of the sample was measured, and it was 6 x 10 16 (atoms/cc New ASTM).
  • a P-type silicon single crystal with a diameter of 150 mm and with a straight body length of 100 cm was produced with the same conditions as Example 1, except charging nylon sandwiched between two chemical etched silicon wafers as a carbon dopant into a quartz crucible. After that, a wafer-shaped sample was sliced from the crystal at 100 cm from the top of the straight body. Carbon concentration of the sample was measured, and it was 3 x 10 16 (atoms/cc New ASTM). As mentioned above, by using nylon including carbon and nitrogen as main elements, a carbon- and nitrogen-doped silicon single crystal was produced.
  • the present invention is not limited to the embodiments described above.
  • the above-described embodiments are mere examples, and those having substantially the same structure as technical ideas described in the appended claims and providing the similar functions and advantages are included in the scope of the present invention.
  • the present invention is applicable regardless of crystal orientation, conductivity type, resistivity and so on of a silicon single crystal to be produced.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
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  • Crystals, And After-Treatments Of Crystals (AREA)
EP05727712A 2004-05-10 2005-03-31 Procede de fabrication d'un monocristal de silicium Active EP1746186B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004140032A JP4507690B2 (ja) 2004-05-10 2004-05-10 シリコン単結晶の製造方法及びシリコン単結晶
PCT/JP2005/006254 WO2005108655A1 (fr) 2004-05-10 2005-03-31 Procédé de fabrication d’un monocristal de silicium et monocristal de silicium

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EP1746186A1 true EP1746186A1 (fr) 2007-01-24
EP1746186A4 EP1746186A4 (fr) 2010-01-13
EP1746186B1 EP1746186B1 (fr) 2012-09-12

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US (1) US7909930B2 (fr)
EP (1) EP1746186B1 (fr)
JP (1) JP4507690B2 (fr)
KR (1) KR101073517B1 (fr)
WO (1) WO2005108655A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101121814B1 (ko) 2010-01-25 2012-03-21 주식회사 엘지실트론 단결정 잉곳 제조방법
EP2186929A4 (fr) * 2007-09-07 2015-03-04 Sumco Corp Germe cristallin pour le tirage d'un monocristal de silicium et procédé pour fabriquer ce dernier au moyen du germe cristallin

Families Citing this family (7)

* Cited by examiner, † Cited by third party
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JP4983161B2 (ja) * 2005-10-24 2012-07-25 株式会社Ｓｕｍｃｏ シリコン半導体基板およびその製造方法
JP4805681B2 (ja) * 2006-01-12 2011-11-02 ジルトロニック アクチエンゲゼルシャフト エピタキシャルウェーハおよびエピタキシャルウェーハの製造方法
JP2008087972A (ja) * 2006-09-29 2008-04-17 Covalent Materials Corp シリコン単結晶の製造方法
JP5061728B2 (ja) 2007-05-30 2012-10-31 信越半導体株式会社 シリコン単結晶の育成方法
JP5104437B2 (ja) * 2008-03-18 2012-12-19 株式会社Ｓｕｍｃｏ 炭素ドープ単結晶製造方法
JP5500138B2 (ja) * 2011-08-25 2014-05-21 信越半導体株式会社 炭素ドープシリコン単結晶の製造方法
JP6741179B1 (ja) * 2020-02-18 2020-08-19 信越半導体株式会社 シリコン単結晶の製造方法

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EP1229155A1 (fr) * 2000-04-14 2002-08-07 Shin-Etsu Handotai Co., Ltd Plaquette de silicium, plaquette de silicium epitaxiale, plaquette de recuit et procede de production de ces plaquettes
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JPH11199380A (ja) * 1997-12-26 1999-07-27 Sumitomo Metal Ind Ltd シリコンウエーハ及び結晶育成方法
JPH11312683A (ja) * 1998-04-28 1999-11-09 Sumitomo Metal Ind Ltd 半導体単結晶シリコンの製造方法
JP2001274166A (ja) * 2000-03-27 2001-10-05 Wacker Nsce Corp シリコン単結晶基板及びその製造方法
EP1229155A1 (fr) * 2000-04-14 2002-08-07 Shin-Etsu Handotai Co., Ltd Plaquette de silicium, plaquette de silicium epitaxiale, plaquette de recuit et procede de production de ces plaquettes
US20030106482A1 (en) * 2001-12-06 2003-06-12 Seh America, Inc. High resistivity silicon wafer having electrically inactive dopant and method of producing same

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2186929A4 (fr) * 2007-09-07 2015-03-04 Sumco Corp Germe cristallin pour le tirage d'un monocristal de silicium et procédé pour fabriquer ce dernier au moyen du germe cristallin
KR101121814B1 (ko) 2010-01-25 2012-03-21 주식회사 엘지실트론 단결정 잉곳 제조방법

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Publication number Publication date
JP4507690B2 (ja) 2010-07-21
EP1746186A4 (fr) 2010-01-13
WO2005108655A1 (fr) 2005-11-17
EP1746186B1 (fr) 2012-09-12
KR20070007912A (ko) 2007-01-16
US7909930B2 (en) 2011-03-22
JP2005320203A (ja) 2005-11-17
KR101073517B1 (ko) 2011-10-17
US20070266930A1 (en) 2007-11-22

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